Method of obtaining nitrogen and making compounds therefrom.



T.- L. WILLSON & M. M. 'HAFP. METHOD or OBTAINING NITROGEN AND MAKING comrouuns mam-"Rom. APIfLIOATION FILED APR. 9, 19i0. RENEWED NOV. 29, 1013.

1,08%;774. 1 Patented Jan.20,1914.

H'N ESSES INVENTBHE TI LAN! LLSIJN MMHA FF UNITED STATES PATENT orriou.

THQMAB LEOIEOLD WILLSOIQ' AND MAXIMILLIAN MATTHEUS HAFF, OF OTTAVTA QNT-BIO, CANADA; SAID HAFF ASSIGNOR T SAID WILLSON.

METHOD 'OF QBTAINING NITROGEN AND MAKING COMPOUNDS THEREFROM.

. Appli ation 1 9i sprite, 191.0, fiert l N0. 5%,376-

Our invention relates to an improved method of obtaining nitrogen and the objects of our invention are to manufacture the nitrogen in such a way that the by-product' roduced Will be useful in an industry whicqa may be readily allied with that of manufacturing the nitrogen compounds, and further to obtain the nitrogen as economically and in as pure a form as possible.

The drawing illustrates a sectional elevation of an apparatus which may be used as cyanamid or nitrids.

to carry out the process.

According to the present invention, the nitrogen is obtained by first burning sulfur or a sulfid ore in a confined body of air and the Sulfur compound, in the preferred mode of carrying out the process, is utilized to make the bisulfite liquor used in paper manufacture. The resultant gas from this step is practically airrich in nitrogen, and to remove the remaining small percentage of oxygen it is proposed to passthe air enriched in nitrogen again overheated sulfur or sulfid ore and in order to maintain either of these in a state of combustion it is necessary to apply external heat to consume the smallpercentagc of oxygen in the gaseous mixture. The nitrogen resulting from the process is then directly converted into a form of commercial nitrogen compound such As far as the first part of the process is concerned it is immaterial how the sulfur compound is extracted and utilized. It might under certain conditions be used to form sulfuric'acid in the well known manner, but the formation of the sulfite liquor as above described will be found extremely convenient as in practice a paper factorymay readily be allied with a factory for producing nitrogen compounds.

The first part of the process is identical with that carried out ordinarily to produce bisulfite liquor. According to this process a confinedbody of air is passed over burning sulfur and then either led througha Specification of Letters Patent.

extracted.

iatonted Jan. 20, 1914. Renewed'Noyember 29, 1813. Serial No. 803,858.

tower containing calcium oxid and magneslum oxld or passed through a mixture of lime and water, the reactions for this process being as follows:

The first part of the proccss may be modified if desired by substituting a sullid ore for the sulfur, the substitution having the ad- Vantage that the extraction of oxygen is likely to be mpre complete. \Vith an iron sulfid ore, such as iron pyrites, the first reaction would be:

any well known manner, or in any suitable type of furnace. Otherwise the heat might be applied to the air or gaseous mixture in a suitable regenerative gas lltllXEl. This modification has the further advantage that the ore is oxidized and so brought to a condition in which the mctal may be readily It will thus be.apparent that this stop of the process, which possesses novelty in itself, might be operated alone to form a convcnimit source for the simultaneous production of nitrogen and sulfur compounds and the oxidization of the pyritcs ore.

In using the process in connection with oaier manufacture n'eviousl Y the on] Y )roduct which has been recovered has been the isulfite of calcium (CaO(SO the gaseous mixture of nitrogen with a small percentage of unacted on air, (probably five to twenty-five per cent.) being allowed to escape. According to the present invention this resultant gaseous n; xturc, which may be termed air enriched in nitrogen is passed over a further quantity of heated sulfur, and to maintain the second supply of sulfur or sulfur compound in a state of combustion it is necessary to apply external heat which may be done in any suitable furnace designcd for the purpose. The heat will. cause the sulfur to combine with any residul oxygen in the mixture, to form sulfur dioxid'as before, which maybe separated ml-LO),

Y compoundslin any way diil'erent embodimentsof ourinventlon, with- Y indhe-edope-ofthe claims, could be made construction havin trays; 10 ;for the;

passing nitrogen through ajmase fofi'calcium;

carbidheate'd-teamed-heat;3 L .Beferrin'g'tothe-apparatus which We have ill'uetratedfor carrying-out the process'hereinhefore described, .Aj represents asulfur burner of any usualf-typ'e,' being "of Inuflieand a; stirring -rah le 11 which" the sulfurousm-aterlal maybe maintained in a burning statef =Thejai-renri chedin nitrogen being led in-{through the conduit "12, is drawn through the burner into a conduit 13' bya suitable blower Be, the gasbeing forced by the blowerthrough I thence below the surface of an aqueous s olutionin a'tank'E,

second blower .F and forced beneathithev surface of a second 'aqueous'solution in a tank G both of saidaqueous solutionsbeing adapted to Wash outthe sulfur oxid. From the tank- G the-nitrogen and 'for'cedto any. desired place" of'consumption by suitable means such as blower H It may be mentioned that the step ofthe burning processspecified in the claims' as sulfur in a confined body of air is intend-c ed to include both the case where the sulfur is burned alone and the ease Where a sulfur oreisburn'ed T As many changes could be" made-in the' above process and many'apparently widely .i,oe e,77e

.thereof, it 1s intended thata at present known'i'nin a limiting-sense the atmosphere who the. atmosphere WhlCh cons sts sulfur in a confined body a suitable scrubber C, j

corn-pound; thence it is';drawn by a? gas may be drawn.

ivithout departing the tained "in the accompanying specification shall be interpreted as i What we. claim 1. Theprocess o nsiets burmng sulfur in aconfined body-= :-.0f the-resultant gaseous mixture throu 1' 2,,Th'e proce's' s of obtaining the resultant gaseous mixture throng lutionf containing lirne liquor and then pas'sing.

ture over externally "heated sulfur and the P gthenitrOgenigas;

sigiritor Scope matter conllus'trative, and not air-[and liasin r v a 'llltlOIl 'contaimng limel-ito form' aw lsulfibe" nitrogen from nitrogen from" in burning 'of air and assifng a 6%; to form bis'ulfit'e' I the resultant mix- I 3-. The process of obta ning nitrogen ijrom the atmosphere, which'consiets inppassing may be I burned in the air-' and removing .t

3 A. -Theiproceee of obtaining from atmosphere which consists-in passing air the enriched in nitrogen over externally heated airenrichedin nitrogen over an externally I heated-substance which normal eox'ygen sulfur, removing the oxysnlfur, compound:

and thenrecov'erin the nitrogen. 5.. The process'o the 7 atmosphere which consists in pa ssmg heated air enriched in fur and removing 'the oxysulfu'r formed.

nitrogen over an compound ,In witness --whereof we have hereunto setv ourhands in he presence of two Witnesses;

Y moms tiiorotn WILLSONa v tMAXIMILLIANMATTHEUS 'WVitne'sses': RUssnL S. S AR MQGQELBERTSON.

. obtaining nitrogen from I 

